Synthesis, Crystal Structure and Property of a Series of Supramolecular Polymers Based on Novel 3,5-Dimethyl- 2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl)pyridine Ligand

Solvothermal reactions of 3,5-dimethyl-2,6-bis（3-（pyrid-2-yl）-1,2,4-triazolyl） pyridine （L）, 1,4-benzendicarboxylic acid （H2bdc）, and transitional metal cations of M11 （M = Mn, Co, Cd） in the presence of oxalic acid （H2ox） afford three novel supramolecular polymers （CPs）, namely, {[M2（ox）（L）2][bdc][M2（Hox）2（OH）（H2O）4]·3H2O}n （M = Mn for 1, Co for 2, Cd for 3）. Single-crystal X-ray diffraction analysis reveals that complexes 1-3 are isostructural and the 3D supramolecular structure was connected through non-covalent interactions. With the help of H2ox, the L ligands cheated with center atoms forming a butterfly [M2（ox）（L）2]2＋ building block. The bdc2- ligand linked with the unprecedented [M2（Hox）2（OH）2（H2O）4] units through strong O-H...O hydrogen bonds forming a zigzag chain, which are further connected through π-π interactions between L and bdc2- ligands to form a 3D supramolecular structure. Moreover, elemental analyses, IR, thermogravimetric, PXRD and luminescence have been investigated.

Synthesis,Crystal Structure,and Magnetic Property of One 3D Nickel Coordination Polymer Based on 2-Hydroxy-5-(3',5'-terephthalic acid)Pyridine and 1,4-Bis(1-imdazoly)benzene

One novel nickel coordination polymer, {[Ni（OTP）（bib）1.5（H2O）]·2H2O}n（1, H2 OTP = 2-hydroxy-5-（3＇,5＇-terephthalic acid） pyridine, bib = 1,4-bis（1-imdazoly）benzene）, has been synthesized and characterized by elemental analysis（EA）, IR, powder X-ray diffraction（PXRD）, and thermogravimetric（TG） analyses. The crystal of 1 crystallizes in monoclinic, space group P21/n with a = 12.2860（5）, b = 13.8246（6）, c = 19.0140（8） A, β = 104.3870（1）°, V = 3128.2（2） A3, Z = 4, C32H28N7 Ni O8, Mr = 697.32, Dc = 1.481 g/cm^3, F（000） = 1444 and μ（Mo Kα） = 0.684 mm-1. The final R = 0.0704 and w R = 0.1764 for 5485 observed reflections with I 2σ（I） and R = 0.1087 and wR = 0.2010 for all data. Topology analysis reveals that complex 1 is a 3D 2-fold interpenetrated {4^4·6^6}-nov net based on the 1D [Ni（OTP）]n chain and the 2D [Ni2（bib）3]n sql sheet. And the variable-temperature magnetic susceptibility measurements exhibit weak antiferromagnetic coupling interaction.

Synthesis and Structure of [Cu_2(μ-NO_2)(aepy)_4](ClO_4)_3 (aepy = 2-(2-Aminoethyl)pyridine)

The title compound [Cu2(m-NO2)(aepy)4](ClO4)3 (Cu2C28H40N9Cl3O14, Mr = 960.12, aepy = 2-(2-aminoethyl)pyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group C2/c with cell parameters: a = 21.958(3), b = 12.205(2), c = 15.180(3) ? b = 106.06(1), V = 3909.5(12) ?, Z = 4, Dc = 1.631 g/cm3, F(000) = 1968 and m(MoKa) = 1.368 mm-1. The structure was solved by direct methods and refined by full-matrix least-squares techniques. The final R = 0.0734 and wR = 0.1954 for 1606 observed reflections with I ≥2.0s(I). The crystal structure revealed that the [Cu2(m-NO2)(aepy)4]3+ cation consists of two square-based pyramidal copper (Ⅱ) atoms bridged by one nitrate anion. The distance between the two copper atoms (Cu(1)…Cu(1A)) is 5.373 (2) ?

A New Diiminopyridyl Cobalt Complex [CoCl_2L](L=2,6-Bis(N,N'-bis(2,6-diisopropyl-4-(2,3-dimethyoxylbenzoylamide)phenylimino))pyridine)

The reaction of CoCl2·6H2O with 2,6-bis（N,N＇-bis（2,6-diisopropyl-4-（2,3-dimethy-oxyl-benzoylamide）phenylimino））pyridine（L） afforded the complex [CoCl2L],which was fully characterized by elemental analysis,UV-vis,IR spectroscopy,fluorescence,and X-ray diffraction analysis.The compound is of triclinic system,space group P1 with a = 13.058（3）,b = 13.798（3）,c = 16.695（3） ,α = 98.191（3）,β = 102.792（3）,γ = 101.820（3）°,V = 2815.0（9） 3,Z = 2,F（000） = 1122,μ = 0.45 mm-1,R = 0.061 and wR = 0.1349 for 9842 observed reflections（Ⅰ 〉 2σ（Ⅰ））.The Co（Ⅱ） center adopts a distorted square-pyramidal coordination geometry.The extended structure shows a one-dimensional zigzag double chain linked by hydrogen bonds and π-π stacking interactions.

Coherent-Synchronized Oxidation of Pyridine with Nitrous Oxide to 2,2- and 2,3-Dipyridil

Synthesis of pyridine bases by way of relatively simple transformations with use of cheaper and available raw, is an actual problem. In this aspect the method in which the reactions of hydro-carbons oxidation are induced by nitrous oxide, is of scientific and practical interest. In the present work, the authors report the results of the experiments coherent-synchronized oxidation of pyridine with nitrous oxide to 2,2- and 2,3-dipyridyle.

Syntheses, Crystal Structures and Photoluminescence Properties of Cadmium(Ⅱ) and Nickel(Ⅱ) Complexes with 2-(2-Benzimidazolyl)quinoline

Two novel complexes, [Cd2（BMQU）2Cl4] （1） and [Ni（BMQU）2HPO4]·1.5H2O （2） （BMQU = 2-（2-benzimidazolyl）quinoline）, were synthesized by the hydrothermal method and characterized by elemental analysis, IR, and TG-DTG. The crystal structures were determined by single-crystal X-ray diffraction. Both 1 and 2 crystallize in the triclinic system, space group P . The data for 1： a = 0.8342（7）, b = 0.9226（9）, c = 1.0646（8） nm, α = 90.819（2）, β = 97.466（2）, γ = 98.280（2）°. The Cd（Ⅱ） is coordinated with three chlorine atoms and two nitrogen atoms of a BMQU molecule, generating a distorted square-pyramidal geometry. The dinuclear Cd（Ⅱ） complex is formed by two chlorine bridge bonds, and the one-dimensional chain structure is constructed with the hydrogen bond N-H…Cl and π-π stacking interaction. The data for 2： a = 1.2251（1）, b = 1.2451（1）, c = 1.2868（1） nm, α = 107.510（2）, β = 98.630（1）, γ = 109.921（2）°. The Ni（Ⅱ） is coordinated with four nitrogen atoms of two BMQU molecules and two oxygen atoms of a HPO42-, forming a distorted-octahedral geometry. The two-dimensional layer structure is formed by the hydrogen bonds and π-π stacking interaction between neighboring molecules. Complex 1 shows a strong blue fluorescence emission （λmax= 456 nm） at solid state.

VINYL POLYMERIZATION OF NORBORNENE CATALYZED BY [2-(2-BENZIMIDAZOLYL)-6-((1-ARYLIMINOETHYL)PYRIDYL)]NICKEL CHLORIDE/MAO SYSTEM

The catalytic system of[2-(2-benzimidazolyl)-6-((1-aryliminoethyl)pyridyl)]nickel chloride/MAO(methylalu- minoxane)was found to be good active for vinyl polymerization of norbornene and provided polymers with relative narrow molecular distributions.Various reaction parameters,such as the ratios of nickel precursor to MAO or monomer norbornene, and the nature of the ligands in complexes were carefully investigated to realize their effects on the catalytic activities, polymer molecular weight and molecular we...

A Novel Degradation Pathway of Zn(dmid)(phen)_2 in Pyridine

The light-oxidation degradation processes of Zn(dmid)(phen)_2 ( dmid = 4,5-dimercapto-l, 3-dithiole-2-one, phen = 1,10-phenanthroaline) in pyridine solvent has beenmonitored. It has been found under the light, dmid^(2-) of Zn(dmid)-(phen)_2 in pyridine solutioncould generate NCS~ and NCS^-replaces dmid^(2-) to form Zn(NCS)_2 (phen)_2 simultaneously. Thecrystal structure of Zn(NCS)_2 (phen)_2 has been determined. In the crystal of Zn(NCS)_2 (phen)_2,two NCS~ ligands are arranged in syn-configuration, and there is strong pi-pi interaction betweenthe two adjacent parallel phen.

Synthesis, Characterization and Luminescence of Lanthanide Chloride Complexes with N,N,N',N'-Tetra[(2-benzimidazolyl) methyl]-1,2-Ethanediamine

N,N,N',N'-tetra[(2-benzimidazolyl)methyl]-1,2-ethanediamine (EDTB) lanthanide chloride complexes were prepared (Ln3+=Eu3+, Tb3+ or Gd3+). The results of single crystal X-ray structural analysis show that [(EDTB)GdCl2]Cl(C2H5OH)(H2O)2 crystal is in space group P21 / c with a=8.848(2) ?, b=26.313(5) ?, c=18.929(4) ?, β=97.82(3)o, V=4366(2) ?3, Z=4. The luminescent properties of the terbium and europium complexes have been studied.

Synthesis, Reactions and Characterization of 1,1’-(1,4-Phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(ethan-1-one)

Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.

Structures and luminescence properties of two copper(I) halide complexes featuring 2-(2-benzimidazolyl)-6-methylpyridine

Two new copper（I） halide complexes bearing 2-（2-benzimidazolyl）-6-methylpyridine （Hbmp） and PPh3 ligands, Cu（Hbmp）（PPh3）X （X = Br （1）; I （2））, have been synthesized and characterized. Single-crystal X-ray structure analysis reveals that the halide ligand has a significant impact on the Cu-Npyridyl bond lengths. Complexes 1 and 2 show the solid-state emissions at ambient temperature, varying with the halide bound to the { Cu（Hbmp）（PPh3） } motif, which are perhaps best attributed to the metal-to-ligand charge-transfer （Cu（I） → Hbmp） transition mixed with some ligand-to-ligand charge-transfer （X and PPh3 → Hbmp） character.

N-(2-Phenoxy)ethyl imidazo[1,2-a]pyridine-3-carboxamides containing various amine moieties:Design,synthesis and antitubercular activity

Seven 2,6-disubstituted N-(2-phenoxy)ethyl imidazo[1,2-a]pyridine-3-carboxamide series containing various amine moieties were designed and synthesized as new anti-TB agents.Many of them show excellent in vitro activity against both drug-sensitive MTB strain H37Rv and two MDR-MTB clinical isolates(MIC:<0.002-0.030 μg/mL).Compounds 2f,5e and 5g display acceptable safety and pharmacokinetic profiles,opening a new direction for further development.

One Novel Tetranuclear Copper Cluster by 2-(1H-Pyrazol-3-yl)pyridine:Synthesis, Structure and Properties

A novel tetranuclear copper cluster[Cu4(μ-L)6Cl2]was constructed by 2-(1H-pyrazol-3-yl)pyridine(HL)under hydrothermal conditions,and structurally concluded by single-crystal X-ray diffractions,elemental analyses and IR spectra.The title complex 1 was of triclinic system,space group■,C24H18ClCu2 N9,Mr=595.01,a=9.6497(13),b=11.4133(7),c=13.0919(15)?,α=99.166(7),β=108.707(11),γ=111.974(9)°,V=1200.7(2)?3,Z=2,Dc=1.997 g/cm^3,F(000)=706,μ(MoKα)=3.203 nm-1,Rint=0.0404,R=0.0536 and wR=0.1490 for4890 observed reflections with I>2σ(I).In this structure,complex 1 was the unimolecule with unprecedented tetranuclear cluster,which was expanded into a 2D network by wide-ranging C-H…Cl intermolecular hydrogen bonds and further exhibited a 3D supramolecular architecture based onπ-πstacking interactions.In addition,the complex was thermally stable up to 300℃and the solid state fluorescent property of 1 was examined and compared with the ligand.

三棱的化学成分研究

目的:研究三棱Sparganium stoloniferumBuch.-Ham.的化学成分。方法:采用硅胶柱层析,Sephadex LH-20,ODS C-18,重结晶等方法,根据理化性质和光谱鉴定化合物的结构。结果:从三棱中得到8个化合物,分别为棕榈酸(1),5-羟甲基糠醛(2),6,7,10-三羟基-8-十八烯酸(3),棕榈酸单甘油酯(4),5-Hydroxy-2-(hydroxymethyl)pyridine(5),β-谷甾醇(β-sitosterol)(6),β-胡萝卜苷(daucosterol)(7),Betulinic acid(8)。结论:化合物5,8为首次从该植物中分离得到。

天然活性化合物羟基白藜芦醇中间体的制备研究

白藜芦醇（Resveratrol,3,4＇,5-trihydroxy-trans-stil-bene）即反式3,4＇,5-三羟基茋,广泛存在于虎杖、葡萄、花生等多种植物中。白藜芦醇作为一种重要的植物抗毒素,具有多种医疗保健生理活性作用,如抗菌、抗氧化、抗癌、抗血小板凝聚、抗艾滋病活性等[1～5]。被誉为继紫杉醇后的第二大抗癌药物。